An eco-friendly extraction method to obtain pectin from passion fruit rinds (Passiflora edulis sp.) using subcritical water and pressurized natural deep eutectic solvents.

This work evaluated the efficiency of Subcritical Water Extraction (SWE) and Pressurized Natural Deep Eutectic Solvents (P-NaDESs) under different temperatures (100, 120, 140 and 160 °C) in obtaining pectin from Passion Fruit Rinds (PFR) and its residual biomass (PFR - UAPLE), and compare the results with those of Conventional Extraction (CE). The highest pectin yields, 19.1 and 27.6 %, were achieved using P-NaDES (Citric Acid:Glucose:Water) at 120 °C for PFR and its PFR-UAPLE, respectively. Regarding the Degree of Esterification (DE), pectin obtained with SWE and CE had DE below 50 %, while with P-NaDES (Citric Acid: Glucose:Water), DE was above 50 %. Higher Molecular Weights (MW) (98 and 81 kDa) were obtained with SWE and P-NaDES from PFR compared to PFR-UAPLE and CE. Galacturonic acid was the most abundant (74 to 78 %) monosaccharide obtained by SWE. In terms of morphology, water extraction provided pectin with more uniform textures, whereas extraction with acidified mixtures led to more heterogeneous surfaces. Overall, comparing SWE and P-NaDES, the obtained pectins differed in terms of monomeric composition, MW and DE. These results indicate that pectins obtained by both methods can have different applications depending on their structural characteristics.

Deep eutectic solvents as an alternative for extraction of flavonoids from soybean (Glycine max (L) Merrill) and okara: An experimental and computational approach based on COSMO-SAC model.

In this study, different Deep Eutectic Solvents based on choline chloride ([Ch]Cl) with carboxylic acids, sugars, and glycerol, were investigated as alternative solvents for the extraction of flavonoids from soybean and okara. Initially, the COSMO-SAC was investigated as a tool in solvent screening for the extraction of flavonoids. Experimental validation was performed using total flavonoid analysis with the solvents that showed greater interaction with the solutes. The extracts obtained from soybean and okara using the DES [Ch]Cl:acetic acid added with 30 % water showed the highest total flavonoid content, 1.05 mg eq. of catechin/g dry soybean and 0.94 mg eq. of catechin /g dry okara, respectively. For phenolic compound extraction, [Ch]Cl: acetic acid DES extracted approximately 1.16 mg GAE/g of soybean and 0.69 mg GAE/g of okara. For antioxidant activity, soybean and okara extracts obtained with [Ch]Cl: acetic acid showed FRAP results of 0.40 mg Trolox/mL of extract and 0.45 mg Trolox/mL of extract, respectively. In addition, the isoflavones daidzein, genistein, glycitein, daidzin, genistin, and glycitin were identified and quantified in the soybean and okara extracts obtained with DES [Ch]Cl: acetic acid with 30% water, totaling 1068.05 and 424.32 µg total isoflavones/g dry sample. Therefore, The COSMO-SAC model was a useful tool in solvent screening, saving time and costs. Also, DES can be an alternative solvent for extracting flavonoids to replace conventional organic solvents, respecting current environmental and human health concerns.

Capsicum chinense var. BRS Moema: chemical characterization by HPLC-ESI-MS/MS and antiproliferative screening.

Capsiate and phenolics present in the free, esterified, glycosylated, and insoluble-bound forms of BRS Moema peppers were characterized and quantified using UHPLC-ESI-MS/MS. Additionally, the in vitro antiproliferative activity of BRS Moema extract was evaluated. The peppers showed considerable quantities of capsiate and phenolic compounds. Esterified phenolics were the main fraction, followed by the insoluble-bound fraction, indicating that relying solely on the extraction of soluble phenolics may underestimate the total phenolic content. Among the fourteen phenolics identified in extract fractions, gallic acid was the major constituent. Phenolic fractions displayed high antioxidant capacity by TEAC and ORAC assays. Nevertheless, the correlation between phenolic compounds and antioxidant activity suggested that other bioactive or phenolic compounds may contribute to the overall phenolic compounds and antioxidant capacity of the obtained fractions. Concerning the antiproliferative activity, the extract did not exhibit any effect on cell proliferation within the evaluated concentration range. These findings indicated that BRS Moema peppers can serve as a rich source of phenolic compounds. Therefore, fully utilizing them could bring advantages to the food and pharmaceutical industries, as well as to consumers and producers.

Standardization proposal to quality control of propolis extracts commercialized in Brazil : A fingerprinting methodology using a UHPLC-PDA-MS/MS approach.

Propolis is a rich source of known and largely explored bioactive compounds with many pharmacological properties. It is used in several commercialized products, such as propolis-enriched honey, candies, mouth and throat sprays, soaps, toothpaste, and skin creams. However, the great diversity of propolis products and different types make the standardization of realistic quality control procedures challenging. Moreover, the extraction of propolis bioactive compounds depends on the technique and the solvent used. In Brazil, the Ministry of Agriculture, Livestock, and Supply (MAPA) set standards to establish commercialized propolis extracts' identity and quality. In addition, according to legislation, propolis extracts must present the main classes of phenols at 200 and 400 nm on the UV spectrum. Still, it is not specified which analysis method should be used to guarantee feasible quality control of the commercialized samples. For this, we proposed a new fast UHPLC-PDA-MS/MS method for analysis and quantification of propolis phenolic compounds. Moreover, we hypothesize that there is no efficient monitoring regarding the quality of the propolis extracts sold in Brazilian stores. Therefore, the present study aimed to perform quality control of 17 Brazilian propolis extracts produced in the Southeast region (green or brown - the most representative samples). The dry extract content (% g/mL), oxidation index (seconds), total flavonoids, and phenolics (% m/m) of each sample were compared with legislation. We conclude that using the UHPLC-PDA method and the investigation that allowed the comparison with the current legislation efficiently practical problems in the commercialization of propolis extracts. However, of the 17 analyzed samples, 6 did not meet the desired the recognized standards, denoting a lack of supervision and efficient quality control, which highlights a dangerous situation regarding the commercialization of this critical product used in several industrial fields, mainly in the food and pharmaceutical sector.

Systemic antioxidant and anti-inflammatory effects of yellow passion fruit bagasse extract during prostate cancer progression.

We evaluated the impact of yellow passion fruit (Passiflora edulis sp.) bagasse extract (PFBE) administration in systemic oxidative and inflammatory parameters in vivo, considering prostate cancer progression in transgenic mice (TRAMP). Piceatannol, scirpusin-B, dicaffeoylquinic acid, citric acid, and (+)-catechin were identified in PFBE, and the extract showed high in vitro antioxidant capacity. Some alterations in systemic parameters were verified during prostate cancer progression, as the increase in ALT and MDA levels, and SOD and GPx activities in the plasma. In the liver, higher MDA, TNF-α, and NF-κB levels, and GR and GPx activities were verified. Compared to their respective controls, the short- and long-term PFBE administration reduced MDA levels in the liver and plasma. The long-term treatment increased the catalase activity in the plasma, while the short-term treatment increased the hepatic SOD and catalase activities. Still, a reduction in hepatic TNF-α and NF-κB levels was verified after long-term treatment. PRACTICAL APPLICATIONS: Prostate cancer progression is associated with changes in systemic redox status and inflammation markers. Moreover, the intake of polyphenols with antioxidant properties, besides delaying prostate carcinogenesis, may improve the systemic antioxidant defenses and inflammatory response. In vitro studies pointed to a promising antioxidant and anti-inflammatory potential of yellow passion fruit bagasse. However, in vivo studies are scarce. Our results provided information about in vivo impacts of PFBE oral consumption on antioxidant defense and inflammation, indicating its potential as an adjuvant during the initial steps of prostate cancer.

Comparison of different extraction methods of Brazilian "pacová" (Renealmia petasites Gagnep.) oilseeds for the determination of lipid and terpene composition, antioxidant capacity, and inhibitory effect on neurodegenerative enzymes.

Pacová (Renealmia petasites Gagnep.) is a Brazilian native plant, usually cultivated in south regions of the country. Pacová was previously reported concerning their possible health benefits, mostly from folk medicine. However, only few works relates the health benefits with the composition of the fruit parts. In this context, this work aimed to bring, for the first time in literature, the chemical characterization in respect to lipid and terpene composition of R. petasites oilseed, performed by three different extraction methods (supercritical fluid extraction (SFE) with CO2, Soxhlet with petroleum ether (SOX), and maceration with hexane (MAC)). SFE was most selective for MUFAs, PUFAs, sesqui- and diterpenes. The main terpene identified in all extracts was 2-carene. The extracts presented poor AChE inhibition, and SOX presented potential inhibitory effect against lipoxygenase activity. Overall, R. petasites oilseed is a natural source of terpenes and their potential health benefits are highly encouraged to be investigated.

Selective Extraction of Piceatannol from Passiflora edulis by-Products: Application of HSPs Strategy and Inhibition of Neurodegenerative Enzymes.

Passiflora edulis by-products (PFBP) are a rich source of polyphenols, of which piceatannol has gained special attention recently. However, there are few studies involving environmentally safe methods for obtaining extracts rich in piceatannol. This work aimed to concentrate piceatannol from defatted PFBP (d-PFBP) by means of pressurized liquid extraction (PLE) and conventional extraction, using the bio-based solvents selected with the Hansen solubility parameters approach. The relative energy distance (Ra) between solvent and solute was: Benzyl Alcohol (BnOH) < Ethyl Acetate (EtOAc) < Ethanol (EtOH) < EtOH:H2O. Nonetheless, EtOH presented the best selectivity for piceatannol. Multi-cycle PLE at 110 °C was able to concentrate piceatannol 2.4 times more than conventional extraction. PLE exhibited a dependence on kinetic parameters and temperature, which could be associated with hydrogen bonding forces and the dielectric constant of the solvents. The acetylcholinesterase (AChE) and lipoxygenase (LOX) IC50 were 29.420 µg/mL and 27.682 µg/mL, respectively. The results reinforce the demand for processes to concentrate natural extracts from food by-products.

Impregnation of passion fruit bagasse extract in alginate aerogel microparticles.

Passion fruit bagasse extract (PFBE) is a rich source of polyphenols, including piceatannol. This work produced alginate (1, 2, 3 wt%) aerogel and investigated the impregnation of gallic acid (GA) and PFBE in alginate aerogel microparticles. The microparticles of ca. 100 µm in diameter were obtained by emulsion-gelation method, submitted to solvent exchange, wet impregnation (WI) and supercritical drying. Alginate aerogels derived from 1 wt% solution led to a higher GA loading and, therefore, this formulation was used to impregnate PFBE. The loading of PFBE, total phenolic, and piceatannol contents based on grams of raw aerogel were 0.62 g, 10.77 mg, and 741.85 µg, respectively, which means a loading efficiency of total phenolics and piceatannol of 47.1% and 34.7%. DSC analysis and X-ray diffraction showed that particles behave as amorphous materials and ORAC assay revealed that impregnated aerogel microparticles presented antioxidant capacity. Alginate aerogel microparticles presented as an appropriated material for drug loading, whereas WI and supercritical drying demonstrated to be useful techniques to load PBBE in aerogels.

Vitamin C in camu-camu [Myrciaria dubia (H.B.K.) McVaugh]: evaluation of extraction and analytical methods.

Camu-camu, a typical Amazonian fruit, is known for the high vitamin C content of the peel and pulp. As vitamin C is widely used in the food, pharmaceutical, and cosmetics industries, it is of interest to study new sources, extraction techniques, and analytical methods for the identification and quantification of this compound. Here, evaluation was made of extraction and quantification methods, as well as the differences in vitamin C content according to the origin and part of the camu-camu fruit. The extraction techniques studied were pressurized liquid extraction (PLE), acid extraction, and maceration. The analytical methods evaluated were titrimetry and chromatography. Camu-camu samples were obtained from different regions, and the peel and pulp were studied separately. Acid extraction using sulfuric acid as solvent provided the highest vitamin C yields, while PLE, as a completely clean technique, proved to be a promising alternative for the recovery of ascorbic acid (L-AA). The application of an ultra-high performance liquid chromatography methodology (UHPLC-DAD) enabled the fast identification and quantification of L-AA and dehydroascorbic acid (DHAA), with high resolution, sensitivity, and specificity. The results obtained using the chromatographic and titration methods were not significantly different (p < 0.05), indicating that titrimetry is useful for routine analyses. L-AA and DHAA were found in the peel, but only L-AA was found in the pulp. The variation of vitamin C content among the lots could be explained by the edaphoclimatic conditions. The combination of a clean extraction technique and a fast analytical method is a promising approach for the determination of vitamin C in food products.

Recovery of anthocyanins from residues of Rubus fruticosus, Vaccinium myrtillus and Eugenia brasiliensis by ultrasound assisted extraction, pressurized liquid extraction and their combination.

This work investigated the extraction efficiency of polyphenols (anthocyanins) from blackberry, blueberry and grumixama residues using combined ultrasonic assisted extraction (UAE) and pressurized liquid extraction (PLE) (UAE+PLE). The performance of UAE+PLE was compared to those achieved by the isolated PLE and UAE methods and conventional Soxhlet extraction. The effects of the extraction methods and solvents (acidified water pH 2.0, ethanol+water 50% v/v and ethanol+water 70% ethanol v/v) on total phenolics content, anthocyanin composition and antioxidant capacity of extracts were investigated by a full factorial design. The extraction efficiency for total phenolics and antioxidant capacity in decreasing order was: UAE+PLE>PLE≈Soxhlet>UAE, and for anthocyanins it was: Soxhlet≈UAE>UAE+PLE>PLE, using hydroethanolic mixtures as solvents. Extractions with acidified water and ultrasound were not effective to recover phenolics. Two, four and fourteen anthocyanins were identified in the extracts from grumixama, blackberry and blueberry, respectively.

Supercritical fluid extraction from spent coffee grounds and coffee husks: antioxidant activity and effect of operational variables on extract composition.

The present study describes the chemical composition and the antioxidant activity of spent coffee grounds and coffee husks extracts, obtained by supercritical fluid extraction (SFE) with CO(2) and with CO(2) and co-solvent. In order to evaluate the high pressure method in terms of process yield, extract composition and antioxidant activity, low pressure methods, such as ultrasound (UE) and soxhlet (SOX) with different organic solvents, were also applied to obtain the extracts. The conditions for the SFE were: temperatures of 313.15K, 323.15K and 333.15K and pressures from 100 bar to 300 bar. The SFE kinetics and the mathematical modeling of the overall extraction curves (OEC) were also investigated. The extracts obtained by LPE (low pressure extraction) with ethanol showed the best results for the global extraction yield (X(0)) when compared to SFE results. The best extraction yield was 15±2% for spent coffee grounds with ethanol and 3.1±04% for coffee husks. The antioxidant potential was evaluated by DPPH method, ABTS method and Folin-Ciocalteau method. The best antioxidant activity was showed by coffee husk extracts obtained by LPE. The quantification and the identification of the extracts were accomplished using HPLC analysis. The main compounds identified were caffeine and chlorogenic acid for the supercritical extracts from coffee husks.

Supercritical fluid extraction of peach (Prunus persica) almond oil: process yield and extract composition.

Peach kernels are industrial residues from the peach processing, contain oil with important therapeutic properties and attractive nutritional aspects because of the high concentration of oleic and linoleic acids. The extraction method used to obtain natural compounds from raw matter is critical for product quality definition. Thus, the aim of this work was to compare peach almond extraction yields obtained by different procedures: soxhlet extractions (Sox) with different solvents; hydrodistillation (HD); ethanolic maceration (Mac) followed by fractionation with various solvents, and supercritical fluid extraction (SFE) at 30, 40 and 50 degrees C and at 100, 200 and 300bar, performed with pure CO(2) and with a co-solvent. The extracts were evaluated with respect to fatty acid composition (FAC), fractionated chemical profile (FCP) and total phenolic content (TPC). The Sox total yields were generally higher than those obtained by SFE. The crossover pressure for SFE was between 260 and 280bar. The FAC results show oleic and linoleic acids as main components, especially for Sox and SFE extracts. The FCP for samples obtained by Sox and Mac indicated the presence of benzaldehyde and benzyl alcohol, components responsible for almond flavor and with important industrial uses, whereas the SFE extracts present a high content of a possible flavonoid. The higher TPC values were obtained by Sox and Mac with ethanol. In general, the maximum pressure in SFE produced the highest yield, TPC and oleic acid content. The use of ethanol at 5% as co-solvent in SFE did not result in a significant effect on any evaluated parameter. The production of peach almond oil through all techniques is substantially adequate and SFE presented advantages, with respect to the quality of the extracts due to the high oleic acid content, as presented by some Sox samples.

Valorization of Brazilian vetiver (Vetiveria zizanioides (L.) Nash ex Small) oil.

The valorization of extracts from Brazilian vetiver (Vetiveria zizanioides (L.) Nash ex Small) roots was studied. This study took into account the extraction method, the chemical composition of the extracts, their sensorial characteristics, and the possibility of chemical transformations of the product. The performed extraction methods were hydrodistillation and extraction with supercritical carbon dioxide. Some pretreatment methods were tested on the vetiver roots and evaluated in terms of extraction yield, process time, chemical composition, and sensorial properties. Supercritical carbon dioxide extraction resulted in high yield (3.2%) in significantly less time than the other methods. The chemical compositions of the extracts obtained by the different methods were also compared to those of commercial vetiver oils from other sources, showing that Brazilian samples had a greater acid amount. An extraction in basic medium from Brazilian vetiver oil was done to remove its main acid (zizanoic acid), which was chemically transformed into an alcohol (khusimol) of desirable sensorial properties. Sensory evaluation indicated that the Brazilian volatile oil without acid could be used in perfumery and the extract obtained with supercritical carbon dioxide could have application in food.